采用固相萃取-气相色谱-质谱法测定有机磷农药。
Determination of Organophosphorus Pesticides Using Solid-Phase Extraction Followed by Gas Chromatography-Mass Spectrometry.
机构信息
Center of Management of Laboratory Equipment, Heilongjiang Bayi Agricultural University, No. 5, Xinfeng Road, Daqing City, Heilongjiang Province 163319, China.
Key Laboratory of Functional Inorganic Material Chemistry, Ministry of Education, School of Chemistry and Materials Science, Heilongjiang University, Harbin 150080, China.
出版信息
J Chromatogr Sci. 2022 Jan 1;60(1):1-6. doi: 10.1093/chromsci/bmab033.
In this study, a method was developed for determination of three organophosphorus pesticides (OPPs) using graphene aerogel solid-phase extraction (SPE) combined with gas chromatography-mass spectrometry (GC-MS). The experimental results showed that the target analytes could be extracted on packed SPE cartridges and then eluted with tetrahydrofuran. The final sample solution was analyzed by GC-MS, which demonstrated good linearity between 0.5 and 500 μg L-1 with a correlation coefficient (r) of 0.9991-0.9998. The limits of detection (S/N = 3) and the limits of quantification (S/N = 10) for the three OPPs ranged from 0.38 to 0.82 μg L-1 and 1.32 to 2.75 μg L-1, respectively. The accuracy of the proposed method was evaluated by measuring the recovery of the spiked samples, which ranged from 91.2 to 103.7%, with relative standard deviations of 2.1-7.2%. This method was successfully applied for the determination of the target analytes in water samples taken from tap, wetlands and canal water.
本研究建立了一种利用石墨烯气凝胶固相萃取（SPE）结合气相色谱-质谱联用（GC-MS）测定三种有机磷农药（OPPs）的方法。实验结果表明，目标分析物可在填充 SPE 小柱上萃取，然后用四氢呋喃洗脱。最终的样品溶液通过 GC-MS 进行分析，结果表明在 0.5 至 500μg/L 范围内具有良好的线性关系，相关系数（r）为 0.9991-0.9998。三种 OPPs 的检测限（S/N=3）和定量限（S/N=10）范围分别为 0.38 至 0.82μg/L 和 1.32 至 2.75μg/L。通过测量加标样品的回收率评估了所提出方法的准确性，回收率范围为 91.2%至 103.7%，相对标准偏差为 2.1%至 7.2%。该方法成功应用于测定取自自来水、湿地和运河水的水样中的目标分析物。
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